Aluminium lithium hydride → Azd8055

HRID 218353ノート

反応式

HRID 218353 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH3:7][C@H:8]1[CH2:13][O:12][CH2:11][CH2:10][N:9]1[C:14]1[N:15]=[C:16]([N:36]2[CH2:41][CH2:40][O:39][CH2:38][C@@H:37]2[CH3:42])[C:17]2[CH:23]=[CH:22][C:21]([C:24]3[CH:25]=[CH:26][C:27]([O:34][CH3:35])=[C:28]([CH:33]=3)[C:29](OC)=[O:30])=[N:20][C:18]=2[N:19]=1>C1COCC1>[CH3:7][C@H:8]1[CH2:13][O:12][CH2:11][CH2:10][N:9]1[C:14]1[N:15]=[C:16]([N:36]2[CH2:41][CH2:40][O:39][CH2:38][C@@H:37]2[CH3:42])[C:17]2[CH:23]=[CH:22][C:21]([C:24]3[CH:25]=[CH:26][C:27]([O:34][CH3:35])=[C:28]([CH2:29][OH:30])[CH:33]=3)=[N:20][C:18]=2[N:19]=1

参加物

4

反応物 2

HCID 21226445Aluminium lithium hydride2 回HCID 59703378HCID 59703378、化合物

生成物 1

HCID 25262965Azd8055収率 96.2%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of lithium aluminium hydride (2M solution in THF, 1.01 mL, 2.01 mmol) was added to a solution of methyl 5-{2,4-bis[(3S)-3-methylmorpholin-4-yl]pyrido[2,3-d]pyrimidin-7-yl}-2-methoxybenzoate (1.47 g, 2.68 mmol) in THF (19.8 mL) at 0° C. under an atmosphere of nitrogen. After 60 minutes, further lithium aluminium hydride (2M solution in THF, 0.67 mL, 1.34 mmol) was added and the solution allowed to stir at RT for 900 minutes. The resulting solution was quenched by the addition of water (11.76 mL) and extracted with ethyl acetate (22 mL). On evaporation of the ethyl acetate, 1.2 g of (5-{2,4-bis[(3S)-3-methylmorpholin-4-yl]pyrido[2,3-d]pyrimidin-7-yl}-2-methoxyphenyl)methanol (6) is obtained as a yellow solid.

後処理

  1. customThe resulting solution was quenched by the addition of water (11.76 mL)
  2. extractionextracted with ethyl acetate (22 mL)
  3. customOn evaporation of the ethyl acetate

出典と根拠

ORDレコード
ord-5801a18097ec4e94b2964a4223ec5a7d
出典データセット
uspto-grants-2012_06
特許番号
US08198441B2

反応ノート

読み込み中…